WO2016200111A1 - Appareil de distillation - Google Patents

Appareil de distillation Download PDF

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Publication number
WO2016200111A1
WO2016200111A1 PCT/KR2016/005981 KR2016005981W WO2016200111A1 WO 2016200111 A1 WO2016200111 A1 WO 2016200111A1 KR 2016005981 W KR2016005981 W KR 2016005981W WO 2016200111 A1 WO2016200111 A1 WO 2016200111A1
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WO
WIPO (PCT)
Prior art keywords
fraction
region
distillation
dividing wall
column
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PCT/KR2016/005981
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English (en)
Korean (ko)
Inventor
이성규
신준호
Original Assignee
주식회사 엘지화학
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Application filed by 주식회사 엘지화학 filed Critical 주식회사 엘지화학
Priority to JP2017562665A priority Critical patent/JP6545830B2/ja
Priority to CN201680033688.0A priority patent/CN107743413B/zh
Priority to US15/579,507 priority patent/US10493375B2/en
Publication of WO2016200111A1 publication Critical patent/WO2016200111A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/141—Fractional distillation or use of a fractionation or rectification column where at least one distillation column contains at least one dividing wall
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C11/00—Aliphatic unsaturated hydrocarbons
    • C07C11/02—Alkenes
    • C07C11/08—Alkenes with four carbon atoms
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C11/00—Aliphatic unsaturated hydrocarbons
    • C07C11/12—Alkadienes
    • C07C11/16—Alkadienes with four carbon atoms
    • C07C11/167—1, 3-Butadiene
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C7/00—Purification; Separation; Use of additives
    • C07C7/04—Purification; Separation; Use of additives by distillation

Definitions

  • the present application relates to a distillation apparatus and method for separating the solvent and unreacted monomer used in the polymerization process of the thermoplastic elastomer with high purity and high efficiency.
  • Thermoplastic elastomers such as butadiene rubber, are excellent in wear resistance, flex resistance and cold resistance, and are used in various applications in the chemical industry.
  • the butadiene rubber is polymerized by a solution polymerization method in which a 1,3-butadiene monomer is dissolved in a solvent and then polymerized using a catalyst, and the solvent is recovered from the polymerization solution and then commercialized.
  • a solution polymerization method in which a 1,3-butadiene monomer is dissolved in a solvent and then polymerized using a catalyst, and the solvent is recovered from the polymerization solution and then commercialized.
  • the present application aims to provide a distillation apparatus for separating the solvent and unreacted monomer used in the polymerization process of the thermoplastic elastomer with high purity and high efficiency.
  • the present application relates to a distillation apparatus.
  • Exemplary distillation apparatus in the purification process of a raw material comprising a monomer, for example, a C 4 fraction and a solvent, for example, a C 6 fraction, used in the polymerization of the thermoplastic elastomer
  • a monomer for example, a C 4 fraction
  • a solvent for example, a C 6 fraction
  • the distillation apparatus of the present application as the C 6 fraction is partially discharged from the top and bottom regions of the dividing wall column, the C 4 oil component is discharged from the product outlet region. Can be prevented.
  • the distillation apparatus of the present application as described above, it is possible to provide a temperature and pressure conditions inside the distillation column for distilling the C 6 oil in a specific content range in the top region and the bottom region, and thus, the distillation apparatus of the present application.
  • the solvent and the unreacted monomer used in the polymerization process of the thermoplastic elastomer can be separated and reused in high purity and high efficiency.
  • FIG. 1 exemplarily shows a distillation apparatus according to an embodiment of the present application.
  • the distillation apparatus of the present application includes a distillation column 100 having a condenser 102, a reboiler 103, and a separation wall 101.
  • the distillation column 100 may be a dividing wall distillation column 100.
  • the dividing wall distillation column 100 is a device designed for distillation of the raw material F 1-1 including three components of low boiling point, middle boiling point, and high boiling point, and is similar in terms of thermodynamic distillation column (Petlyuk column). Device.
  • the heat-comprising distillation column primarily separates low boiling point and high boiling point materials from the preliminary separator, and the top and bottom portions of the preliminary separator are introduced into the feed stage of the main separator, respectively. It is designed to separate each one.
  • the dividing wall distillation column 100 is a form in which the preliminary separator is integrated into the main separator by installing the dividing wall 101 in the tower.
  • the design structure and operation conditions of the distillation column are very limited, and in particular, the design structure of the number of stages, feed stage and outlet of the distillation column according to the properties of the compound to be distilled.
  • a dividing wall distillation column designed for separating the solvent and unreacted monomer used in the polymerization process of the thermoplastic elastomer with high purity and high efficiency ( 100 can provide the operating conditions.
  • the specific kind of the dividing wall distillation column 100 that can be used in the distillation apparatus of the present application is not particularly limited.
  • a dividing wall distillation column 100 having a general structure as shown in FIG. 1 may be used, or a distillation column designed to change the position or shape of the dividing wall 101 in the distillation column in consideration of purification efficiency may be used.
  • the number of stages and the inner diameter of the distillation column are not particularly limited, and for example, the number of stages inferred from the distillation curve in consideration of the composition of the raw material F 1-1 may be set.
  • the dividing wall distillation column 100 of the present application may have a structure as shown in FIG. 1. As shown in FIG. 1, the exemplary dividing wall distillation column 100 is divided by a dividing wall 101. In addition, the interior of the dividing wall distillation column 100 is divided into an imaginary dotted line in FIG. 1, an intermediate region including the dividing wall 101, an upper region and a lower portion not including the dividing wall 101. It can be divided into areas. In addition, the intermediate region may be divided into a raw material supply region 120 and a product outlet region 130 divided by the dividing wall 101.
  • the dividing wall distillation column 100 may include a top region 110 in which a low boiling point flow is discharged, a bottom region 140 in which a high boiling point flow is discharged, and a raw material supply region in which a raw material F 1-1 is introduced. 120) and a product outlet region 130 through which the product flows out.
  • “Top column” of the dividing wall distillation column 100 means the top portion of the column of the dividing wall distillation column 100, and may be included in the upper region of the dividing wall distillation column 100 described above.
  • “Top bottom” of 100 means the bottom portion of the column of the dividing wall distillation column 100, and may be included in the lower region of the dividing wall distillation column 100 described above.
  • the upper region is used in the same sense as the top region 110, and the lower region is used in the same sense as the top region 140.
  • the "condenser” is a device installed separately from the distillation column, and may mean an apparatus for cooling the material flowing out of the main body in contact with the cooling water introduced from the outside.
  • the condenser 102 of the distillation apparatus may be a device for condensing the overhead stream (F 1-2 ) flowing out of the overhead region 110 of the dividing wall distillation column (100).
  • the "reboiler” is a heating device installed outside the distillation column, it may mean a device for heating and evaporating the high boiling point flow again.
  • the reboiler 103 of the distillation apparatus may be a device for heating the top flow (F 1-3 ) flowing out from the bottom region 140 of the dividing wall distillation column (100).
  • the raw material supply region 120 and the product outlet region 130 may be separated or isolated from each other by the dividing wall 101. Accordingly, the flow in the raw material supply region 120 and the flow in the product outlet region 130 may be prevented from being mixed with each other.
  • the term "separation or isolation” means that the flow in each region flows or exists independently in the region divided by the separating wall 101.
  • the dividing wall 101 of the dividing wall distillation column 100 is included in the middle region of the dividing wall distillation column 100.
  • the partition wall 101 when the partition wall 101 is calculated based on the theoretical number of stages of the dividing wall distillation column 100, 40 to 60% of the total theoretical number calculated based on the column top, preferably 42 to 55%. More preferably, 44 to 50%.
  • theoretical stage number means the number of virtual regions or stages in which the two phases, such as gaseous phase and liquid phase, are balanced with each other in the dividing wall distillation column 100. Since the dividing wall 101 is included in the dividing wall distillation column 100 within the above range, it is possible to effectively block the flow in the raw material supply region 120 and the flow in the product outlet region 130. In addition, it is possible to prevent the low-boiling components mixed in the product flow (F 1-4 ) flowing out of the product outlet region 130 to flow out.
  • the dividing wall distillation column 100 includes a raw material supply port 121 positioned in the raw material supply region 120, and the raw material supply port 121 includes C 4 oil and C 6.
  • the raw material F 1-1 containing the oil is introduced.
  • the C 4 fraction is a monomer component used for the polymerization of the thermoplastic elastomer, in particular, an unreacted monomer component after the polymerization, 1,3-butadiene, 1-butene, n-butane, iso-butane, It may include one or more selected from the group consisting of trans-2-butene and cis-2-butene, but is not limited thereto.
  • the C 4 fraction when the thermoplastic elastomer is butadiene rubber, the C 4 fraction may be 1,3-butadiene.
  • the C 6 fraction is a solvent component in which the monomer is dissolved, and may include one or more selected from the group consisting of n-hexane, c-hexane, and iso-hexane, but is not limited thereto.
  • the C 6 fraction may be n-hexane.
  • the raw material F 1-1 including the C 4 fraction and the C 6 fraction flows into the raw material supply port 121 located in the raw material supply region 120 of the dividing wall distillation column 100
  • the introduced raw material (F 1-1 ) is the introduced raw material (F 1-1 ) is the bottom flow (F 1-3 ) flowing out from the bottom bottom region 140, the top flow flowing out from the top region (110) F 1-2 ) and a product flow (F 1-4 ) exiting the product outlet port 131 located in the product outlet region 130, respectively.
  • a column top flow F 1-2 which is a relatively low boiling point component among the components included in the raw material F 1-1, may flow out.
  • a bottom bottom flow F 1-3 which is a relatively high boiling point component, from the components included in the raw material F 1-1 may flow out.
  • a product flow F 1-4 which is a relatively middle boiling point component, may be discharged among the components included in the raw material F 1-1 .
  • low boiling point flow refers to a stream in which a relatively low boiling point component is rich among raw material streams including three components of low boiling point, middle boiling point, and high boiling point component, and the low boiling point flow is, for example, separated. It means a flow flowing out of the top region 110 of the wall distillation column (100).
  • high boiling point flow refers to a stream in which a relatively high boiling point component is rich among raw material streams including three components of low boiling point, middle boiling point, and high boiling point component, and the high boiling point flow is, for example, A relatively high boiling point component flowing out of the bottom region 140 of the dividing wall distillation column 100 means a rich flow.
  • the “medium boiling point flow” refers to a rich flow of a component having a boiling point between a low boiling point component and a high boiling point component in a raw material stream including three components of a low boiling point, a middle boiling point and a high boiling point component.
  • the flow means, for example, the flow flowing out of the product outlet port 131 of the product outlet region 130 of the dividing wall distillation column 100.
  • the term “rich flow” refers to flow out from the top region 110 of the dividing wall distillation column 100 rather than the content of the low boiling point component, the high boiling point component and the middle boiling point component contained in the raw material F 1-1 .
  • the lower boiling point component included in the stream, the high boiling point component included in the stream flowing out of the bottom region 140, and the middle boiling point component included in the stream flowing out of the product outlet region 130 mean higher flows.
  • Each content represented by the middle boiling point component included may mean a flow of 50% by weight, 80% by weight, 90% by weight, 95% by weight or 99% by weight or more.
  • the top boiling flow (F 1-2 ) of the low boiling point stream and the dividing wall distillation column 100 may be used in the same sense, and the high boiling point flow and the bottom bottom flow (F 1-3 ) of the dividing wall distillation column 100. ) May be used in the same sense, and the product boiling point F 1-4 of the middle boiling point stream and the dividing wall distillation column 100 may be used in the same sense.
  • the dividing wall distillation column (100) comprises a product outlet port (131), in the product outlet port.
  • the product stream flows out.
  • the product outlet port 131 may be located in the product outlet region 130 of the dividing wall distillation column 100.
  • the product outlet port 131 may be located above or above the raw material supply port 121.
  • the raw material supply port 121 is 55 to 85%, 55 to 55 of the total theoretical number calculated based on the column top, when the theoretical number of stages of the dividing wall distillation column 100 is calculated based on the column top 84% or from 60 to 85%.
  • the product outlet port 131 is 40 to 55%, 43 to 55% of the total theoretical number calculated based on the column top, when the theoretical number of stages of the dividing wall distillation column 100 is calculated based on the column top May be located between 40 and 50%.
  • the theoretical stage of the dividing wall distillation column 100 is 100 stages
  • one stage of the dividing wall distillation column 100 corresponds to a tower top and 100 stages corresponds to a column bottom
  • the raw material supply port 121 is 55 to 85 degrees. It may be located at the stage, and the product outlet port 131 may be located at 40 to 55 stage.
  • the product outlet port 131 is located above the raw material supply port 121, the component having a higher boiling point than the C 6 fraction which has the greatest influence on the purity of the C 6 fraction obtained in the product outlet region.
  • the raw material (F 1-1 ) is supplied to the raw material of the dividing wall distillation column 100 as shown in FIG. It may flow into the raw material supply port 121 of the region 120.
  • the raw material F 1-1 including the C 4 fraction and the C 6 fraction introduced into the raw material supply port 121 of the raw material supply region 120 is an oil having a higher boiling point than the C 6 fraction, for example, C 4, a bottom stream comprising dimer and trimers of the C 4 fraction of fraction (F 1-3), wherein the C 4 fraction, e.g., the overhead stream containing 1,3-butadiene (F 1-2), and the It may be separated off into a product stream (F 1-4 ) comprising a C 6 fraction, for example n-hexane, and discharged.
  • the bottom stream F 1-3 flowing out of the bottom region 140 of the dividing wall distillation column 100 passes through the reboiler 103 and the bottom stream F 1-3 passed through the reboiler 103. Some or all of) may be introduced into the bottom region 140 to be refluxed into the dividing wall distillation column 100 or may be stored as a product.
  • the overhead flow (F 1-2 ) flowing out of the overhead region 110 of the dividing wall distillation column 100 passes through the condenser 102 and the overhead flow (F 1-2 ) passed through the condenser 102.
  • Some or all of) may be introduced into the column top region 110 to be refluxed to the dividing wall distillation column 100, or stored as a product, the product outlet port of the product outlet area 130 of the dividing wall distillation column 100
  • the product stream F 1-4 exiting 131 can be stored as a product.
  • a portion of the C 6 fraction included in the product stream (F 1-4 ) may be included in the overhead stream and the bottom stream to flow out.
  • the introduced raw material is the C 6 fraction and the column bottom flow (F 1-3), and the C 4 fraction and an overhead stream (F 1-2), and C 6 product stream comprising a fraction containing the C 6 fraction containing the higher boiling point fraction than the C 6 fraction (F 1-4 ) can be separated and spilled.
  • the distillation apparatus of this application the overhead stream (F 1-2) in the C 6 control an amount of 1 to 20 parts by weight relative to the total components contained in the amount of oil in the overhead stream (F 1-2) may be, the column bottom flow (F 1-3) the content of the C 6 fraction can be adjusted as part of 85 to 95 parts by weight relative to the total components contained in the column bottom flow (F 1-3) within and, therefore, excellent Separation efficiencies not only separate high purity C 6 fractions but also increase recovery. That is, by adjusting the content of the C 6 fraction contained in the overhead stream (F 1-2 ) and the bottom stream (F 1-3 ) described above, the C 6 fraction, for example, n-hexane, It can be separated effectively and maximize energy savings. In addition, as part of the C 6 fraction in the top and bottom regions of the dividing wall distillation column as described above, it is possible to prevent the C 4 oil component from being discharged from the product outlet region.
  • the overhead stream in the amount of C 6 fraction (F 1-2) is containing from 1 to 20 parts by weight, for example, relative to the total components contained in the overhead stream (F 1-2), 3 to 18 parts by weight, 5 to 16 parts by weight, 7 to 20 may Buil parts by weight or from 8 to 14 parts by weight, the content of the C 6 fraction in the column bottom flow (F 1-3) is contained in the column bottom flow (F 1-3) It may be 85 to 95 parts by weight, for example 85 to 94 parts by weight, 85 to 93 parts by weight, 85 to 92 parts by weight or 85 to 90 parts by weight relative to the total components.
  • the content of n-hexane in the overhead stream (F 1-2 ) is 1 to 20% by weight, for example 3 to 18% by weight, 5 to 16% by weight, 7 to 20% by weight or 8 to 8%. 14% by weight, the content of n-hexane in the bottom stream (F 1-3 ) is 85 to 95% by weight, for example, 85 to 94% by weight, 85 to 93% by weight, 85 to 92% by weight Or 85 to 90% by weight, in this case, the content of 1,3-butadiene in the column top flow (F 1-2 ) of the dividing wall distillation column 100 is 1% by weight or less, 3% by weight or less, or 5 The content of n-hexane in the product stream F 1-4 of the dividing wall distillation column 100 may be 85 wt% or more, 87 wt% or more, or 88 wt% or more.
  • the raw material F 1-1 including the C 4 fraction and the C 6 fraction is introduced into the raw material supply port 121 of the dividing wall distillation column 100.
  • a column including a portion of the C 6 fraction among the components of the raw material F 1-1 and a C 4 fraction which is a relatively low boiling point component is a flow.
  • a stream (F 1-2 ) for example, a stream comprising 1,3-butadiene and n-hexane may be withdrawn, and the overhead column (F 1-2 ) withdrawn is partially passed through condenser (102). Is refluxed to the top region 110 of the dividing wall distillation column 100, and the remaining part may be stored as a product.
  • the column bottom region 140 of the dividing wall distillation column 100 includes a portion of the C 6 fraction among the components of the raw material (F 1-1 ) and a component having a higher boiling point than the C 6 fraction, which is a relatively high boiling point component.
  • the column bottom flow (F 1-3) for example, C 4 flows out into dimers and trimers and the stream comprising the C 4 fraction of n- hexane fraction
  • the said bottom outlet flow (F 1-3) which is Part of the reboiler 103 may be refluxed to the bottom region 140 of the dividing wall distillation column, and the other part may be stored as a product.
  • the C 6 fraction When separating the raw material (F 1-1 ) containing the C 4 fraction and C 6 fraction as described above using the distillation apparatus of the present application, the C 6 fraction to flow out of the top and bottom regions in a specific content range
  • the temperature and pressure conditions inside the distillation column can be controlled to a specific range.
  • the pressure in the top region 110 of the dividing wall distillation column 100 is 3.5 kg / cm 2 g to 4.5 kg / cm 2 g, for example, 3.6 kg / cm 2 g to 4.4 kg / cm 2 g, or 3.7 to 4.3 kg / cm 2 g
  • the pressure of the bottom region 140 of the dividing wall distillation column 100 is 3.63 to 4.7 kg / cm 2 g, for example, 3.65 kg / cm 2 g to 4.6 kg / cm 2 g, or 3.67 kg / cm 2 g to 4.5 kg / cm 2 g.
  • the temperature of the top region 110 of the dividing wall distillation column 100 may be 45 °C to 60 °C, 47 °C to 58 °C, or 49 °C to 56 °C, the top bottom region of the dividing wall distillation column 100
  • the temperature of 140 may be 120 ° C to 140 ° C, 122 ° C to 138 ° C, or 124 ° C to 136 ° C.
  • the reflux ratio of the column top flow (F 1-2 ) refluxed in the column top region 110 of the dividing wall distillation column 100 of the column flow (F 1-2 ) of the dividing wall distillation column 100 may be 4.5 to 8.0. From the thermodynamic point of view, preferably 4.6 to 5.8, or 4.8 to 5.6.
  • the "reflux ratio” means the ratio of the flow rate (kg / hr) refluxed with respect to the outflow flow rate (kg / hr) flowing out from the distillation column (100).
  • the present application also relates to a distillation method for separating the solvent and unreacted monomer used in the polymerization process of the thermoplastic elastomer with high purity and high efficiency.
  • Exemplary distillation method of the present application may be carried out using the above-described distillation apparatus, and therefore, descriptions overlapping with those described in the above-described distillation apparatus will be omitted.
  • the step of flowing the raw material (F 1-1) is the is a step of introducing the raw material (F 1-1) comprising a C 4 fraction and a C 6 fraction, a separate Wall Distillation Column 100, and more specifically, the inner
  • the partition wall 101 is provided at the inside, and the interior is divided into a top region 110 and a bottom region 140 in which the partition wall 101 is not located, and an intermediate region in which the partition wall 101 is located.
  • the intermediate region is a step of flowing into the raw material supply region 120 of the dividing wall distillation column 100 divided into the raw material supply region 120 and the product outlet region 130 divided by the dividing wall 101. .
  • Distillation separating the raw material (F 1-1) has a top area 110, a product outlet area (130 of the separation Wall Distillation Column 100 in the raw material (F 1-1) flows into the raw material supply region 120 And a step of separating and dividing each from the column bottom region 140, and more specifically, separating and distilling the C 4 oil and the C 6 oil from the top region 110 of the distillation column of the distillation column 100. outflow of the product, separating the C 6 fraction from the outlet region 130, and a step in which the C 6 fraction, and separating the higher boiling point fraction than the C 6 fraction flowing out of the bottom region 140 of the column.
  • the distillation step is, for the overhead stream (F 1-2) 1 to 20 parts by weight relative to the total components contained in the amount of C 6 fraction in said overhead stream (F 1-2), for example, , 3 to 18 parts by weight, 5 to 15 parts by weight, 7 to 20 parts by weight or 8 to 14 parts by weight, and the content of the C 6 fraction in the bottom flow (F 1-3 ) is the bottom flow (F 1- 3 to 85 to 95 parts by weight, for example, 85 to 94 parts by weight, 85 to 93 parts by weight, 85 to 92 parts by weight or 85 to 90 parts by weight based on the total components included in, As a result, the C 6 fraction of high purity can be separated with excellent efficiency.
  • the C 6 fraction for example, n-hexane, which flows out into the product stream can be effectively separated. And it can maximize the energy saving effect.
  • each of the steps is organically combined independently, each boundary is not clearly divided according to the order of time, and thus, each of the above steps may be performed sequentially or independently of each other.
  • the method may not be limited to the above steps, since the process may further include a process step that may be conventionally performed in the art before or after each step.
  • the economical efficiency of the process can be improved by reducing the energy consumption and minimizing the size of the distillation apparatus used for the purification of the raw materials.
  • distillation apparatus of the present application it is possible to minimize the energy loss generated during the purification of the raw material containing the monomer and the solvent used in the polymerization process of the thermoplastic elastomer, and distillation apparatus than when using two distillation column It is possible to reduce the installation cost, thereby improving the economics of the process.
  • FIG. 1 exemplarily shows a distillation apparatus according to an embodiment and example of the present application.
  • FIG. 2 is a diagram schematically showing a distillation apparatus used in a comparative example.
  • the butadiene mixture and n-hexane were separated using the distillation apparatus of FIG. 1. Specifically, the raw material of 93 containing 1,3-butadiene and n-hexane is introduced into the raw material supply port located at the 19th stage of the dividing wall column having 30 theoretical stages at a flow rate of 21,269 kg / hr to perform the separation process. Each stream was discharged from the top region, the product outlet region and the bottom region of the dividing wall distillation column.
  • the product flow flowing out at the flow rate of 20,562 kg / hr in the product outlet region was separated by distillation from the product outlet port located at the 15 stage of the dividing wall distillation column having the theoretical stage of 30 stages, and the product containing n-hexane. Stored separately.
  • the operating pressure of the column top region of the dividing wall distillation column was adjusted to 4.0 kg / cm 2 g to 4.1 kg / cm 2 g
  • the operating temperature was adjusted to 56 to 59
  • the operating pressure of the column bottom region is 4.15 kg / cm 2 g to 4.25 kg / cm 2 g and operating temperature were adjusted to 129-132.
  • the operating pressure of the product outflow zone was adjusted to 4.1 kg / cm 2 g to 4.2 kg / cm 2 g, the operating temperature was adjusted to 125 to 127.
  • the reflux ratio of the column top region of the dividing wall distillation column was set to 5.8 to 6.4.
  • the content of the C 6 fraction in the overhead stream was adjusted to 9.9 parts by weight based on the total components contained in the overhead stream, and the content of the C 6 fraction in the tower stream was adjusted to 85 parts by weight relative to the total components included in the tower stream. It became.
  • the operating pressure of the column top region of the dividing wall distillation column is adjusted to 3.6 kg / cm 2 g to 3.7 kg / cm 2 g, the operating temperature to 54 to 58 ° C., and the operating pressure of the column bottom region to 3.85 kg / cm 2 g to 3.95.
  • kg / cm 2 g, operating temperature was adjusted to 123 to 125 °C, except that the operating pressure of the product outflow zone is adjusted to 3.7 kg / cm 2 g to 3.8 kg / cm 2 g, operating temperature to 123 to 125 °C 1,3-butadiene and n-hexane were separated in the same manner as in Example 1.
  • the reflux ratio of the column top region of the dividing wall distillation column was set to 5.6 to 6.2.
  • the content of the C 6 fraction in the overhead stream was adjusted to 9.9 parts by weight based on the total components contained in the overhead stream, and the content of the C 6 fraction in the tower stream was 85 relative to the total components included in the tower stream. It was adjusted by weight.
  • the operating pressure of the column top region of the dividing wall distillation column is 4.3 kg / cm 2 g to 4.4 kg / cm 2 g
  • the operating temperature is adjusted to 60 °C to 63 °C
  • the operating pressure of the column bottom region from 4.55 kg / cm 2 g to 4.65 kg / cm 2 g
  • operating temperature was adjusted to 129 ° C. to 132 ° C.
  • operating pressure of product outflow zone was adjusted to 4.4 kg / cm 2 g to 4.5 kg / cm 2 g
  • 1,3-butadiene and n-hexane were separated in the same manner as in Example 1.
  • the reflux ratio of the column top region of the dividing wall distillation column was set to 7.0 to 7.5.
  • the content of the C 6 fraction in the overhead stream was adjusted to 9.9 parts by weight based on the total components contained in the overhead stream, and the content of the C 6 fraction in the tower stream was 85 relative to the total components included in the tower stream. It was adjusted by weight.
  • Example 2 Same as in Example 1 except that the raw material supply port is located at 25 stages of the dividing wall distillation column having 30 theoretical stages and the product outlet port is located at 13 stages of the dividing wall distillation column having 30 theoretical stages. 1,3-butadiene and n-hexane were separated by the method.
  • the content of the C 6 fraction in the overhead stream was adjusted to 9.9 parts by weight based on the total components contained in the overhead stream, and the content of the C 6 fraction in the tower stream was 85 relative to the total components included in the tower stream. It was adjusted by weight.
  • Example 2 Same as in Example 1 except that the raw material feed port is located at 15 stages of the dividing wall distillation column having 30 theoretical stages and the product outlet port is located at 19 stages of the dividing wall distillation column having 30 theoretical stages. 1,3-butadiene and n-hexane were separated by the method.
  • the content of the C 6 fraction in the overhead stream was adjusted to 9.9 parts by weight based on the total components contained in the overhead stream, and the content of the C 6 fraction in the tower stream was 85 relative to the total components included in the tower stream. It was adjusted by weight.
  • butadiene mixture and n-hexane were separated using a distillation apparatus connected to two distillation columns. Specifically, the raw material of 138 containing 1,3-butadiene and n-hexane was introduced into the first distillation column at a flow rate of 21,269 kg / hr to perform a separation process.
  • the low-boiling stream discharged at a flow rate of 1,451 kg / hr in the top column of the first distillation column was passed through the condenser, partly refluxed to the first distillation column, and the other part was stored as product, and at a flow rate of 20,615 kg / hr in the bottom area of the first distillation column.
  • Part of the discharged stream was recirculated using a reboiler and part was returned to the bottom region of the first distillation column and the other part was introduced to the second column.
  • the middle boiling point stream discharged at the top of the second distillation column at a flow rate of 25,867 kg / hr was condensed using a condenser, partly refluxed to the top of the second distillation column, and the other part was separated into the product, and at the bottom of the second distillation column
  • the high boiling point stream discharged at a flow rate of 23 kg / hr was recirculated to the bottom region of the second distillation column using a reboiler, and part was separated into the product.
  • the temperature of the top of the first distillation column was adjusted to 45 to 65, the pressure is 3.5 kg / cm 2 g to 4.5 kg / cm 2 g, the temperature of the tower bottom is 120 to 140, the pressure is 3.71 kg / cm 2 g to 4.71 kg / cm 2 g was adjusted, the temperature of the top of the second distillation column was 75 to 95, the pressure was adjusted to 0.24 kg / cm 2 g to 0.91 kg / cm 2 g, the temperature of the tower bottom is 92 to 107, the pressure was From 0.4 kg / cm 2 g to 10.7 kg / cm 2 g.
  • the reflux ratio of the column top region of the first distillation column was set to 0.50 to 0.60, the reflux ratio of the column top region of the second distillation column was set to 0.15 to 0.25.
  • the total amount of energy used in the purification process using the distillation apparatus of the embodiment of the present application can be confirmed that the total energy consumption is reduced compared to the total amount of energy used in the purification process using the distillation apparatus of the comparative example. . That is, when separating 1,3-butadiene and n-hexane by the distillation apparatus according to the embodiment of the present application, it is possible to obtain an energy saving effect of up to 54.6% compared to the case of using the distillation apparatus of the comparative example.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

La présente invention concerne un appareil de distillation et un procédé de distillation. L'appareil de distillation de la présente invention permet de réduire au minimum la perte d'énergie survenant dans un procédé de purification d'un matériau brut comprenant un monomère et un solvant qui sont utilisés dans un procédé de polymérisation d'un élastomère thermoplastique, permet de réduire le coût d'installation de l'appareil de distillation par rapport aux situations où deux colonnes de distillation sont utilisées pour la purification, et permet ainsi d'améliorer le rendement économique du procédé.
PCT/KR2016/005981 2015-06-08 2016-06-07 Appareil de distillation WO2016200111A1 (fr)

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CN201680033688.0A CN107743413B (zh) 2015-06-08 2016-06-07 蒸馏装置
US15/579,507 US10493375B2 (en) 2015-06-08 2016-06-07 Distillation device

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US10493375B2 (en) 2019-12-03
CN107743413A (zh) 2018-02-27
JP2018517554A (ja) 2018-07-05
CN107743413B (zh) 2020-03-20
KR20160144102A (ko) 2016-12-16

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